液相色谱-四极杆-飞行时间质谱法筛查苹果汁中6种苯乙胺类新精神活性物质

Screening of 6 kinds of new phenylethylamine psychoactive substances in apple juice by liquid chromatography-quadrupole-time of flight mass spectrometry

中文关键词:  液相色谱-四极杆-飞行时间质谱  QuEChERS  苯乙胺  苹果汁

英文关键词:liquid chromatography-quadrupole-time of flight mass spectrometry  QuEChERS  phenylethylamine  apple juice

中文摘要:

      目的 建立一种液相色谱-四极杆-飞行时间质谱法同时定性筛查苹果汁中的6种苯乙胺类新精神活性物质的方法。方法 样品经10 mL乙腈提取, C18粉末净化, 经C18色谱柱(100 mm×2.1 mm, 2.7 μm)分离, 以10 mmol/L乙酸铵水溶液(0.1%甲酸)和乙腈作为流动相, 进行梯度洗脱, 电喷雾电离, 正离子扫描, 信息依赖性采集(information-dependent acquisition, IDA)模式检测。通过目标物信号的质量偏差、保留时间、同位素分布、二级谱库相似度等因素进行筛查。结果 6种目标物在0.1~50.0 μg/L范围内方法的线性关系良好(r>0.9990), 基质效应均小于20%, 属于弱基质效应; 检出限为5.0 μg/L, 定性筛查综合得分均大于90分, 满足定性确证要求。结论 本方法简单快速、灵敏度高, 可用于苹果汁中6种苯乙胺类新精神活性物质的定性筛查检测。

英文摘要:

      Objective To establish a method for concurrent qualitative screening of 6 kinds of new phenylethylamine psychoactive substances in apple juice by liquid chromatography-quadrupole-time of flight mass spectrometry. Methods The samples were extracted with 10 mL acetonitrile, purified with C18 powder, and separated on a C18 column (100 mm×2.1 mm, 2.7 μm). The 10 mmol/L ammonium acetate aqueous solution (0.1% formic acid) and acetonitrile was as mobile phase, and the elution method was gradient elution. Mass spectrometry methods included electrospray ionization, positive ion scanning and information-dependent acquisition (IDA) mode detection. Screening was conducted by considering multiple factors, including the mass deviation, retention time, isotope distribution characteristics and similarity to the secondary spectrum library of the target signal. Results The 6 kinds of targets showed good linearity (0.1–50.0 μg/L, r>0.9990) with matrix effects was all less than 20%, which could be classified as weak matrix effects. The limit of detection was 5.0 μg/L. The comprehensive scores of the qualitative screening were all above 90 points, meeting the requirements for qualitative confirmation. Conclusion The method is simple, rapid and sensitive, and can be used for the qualitative screening and detection of 6 kinds of new phenylethylamine psychoactive substances in apple juice.